EP2619155B1 - Method for making a porous ceramic element for diffusing a liquid - Google Patents

Method for making a porous ceramic element for diffusing a liquid Download PDF

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EP2619155B1
EP2619155B1 EP10769016.6A EP10769016A EP2619155B1 EP 2619155 B1 EP2619155 B1 EP 2619155B1 EP 10769016 A EP10769016 A EP 10769016A EP 2619155 B1 EP2619155 B1 EP 2619155B1
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Prior art keywords
type
silica
porous
particle size
fines
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German (de)
French (fr)
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EP2619155A1 (en
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Benoît Serge Claude BRAULT
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Exel Industries SA
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Exel Industries SA
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
    • C04B35/18—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in aluminium oxide
    • C04B35/19—Alkali metal aluminosilicates, e.g. spodumene
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01G—HORTICULTURE; CULTIVATION OF VEGETABLES, FLOWERS, RICE, FRUIT, VINES, HOPS OR SEAWEED; FORESTRY; WATERING
    • A01G27/00—Self-acting watering devices, e.g. for flower-pots
    • A01G27/006—Reservoirs, separate from plant-pots, dispensing directly into rooting medium
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
    • C04B35/18—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in aluminium oxide
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/0038—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by superficial sintering or bonding of particulate matter
    • C04B38/0041—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by superficial sintering or bonding of particulate matter the particulate matter having preselected particle sizes
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
    • C04B2111/00793—Uses not provided for elsewhere in C04B2111/00 as filters or diaphragms
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
    • C04B2111/00793—Uses not provided for elsewhere in C04B2111/00 as filters or diaphragms
    • C04B2111/00801—Membranes; Diaphragms
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3427—Silicates other than clay, e.g. water glass
    • C04B2235/3463—Alumino-silicates other than clay, e.g. mullite
    • C04B2235/3472—Alkali metal alumino-silicates other than clay, e.g. spodumene, alkali feldspars such as albite or orthoclase, micas such as muscovite, zeolites such as natrolite
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/349—Clays, e.g. bentonites, smectites such as montmorillonite, vermiculites or kaolines, e.g. illite, talc or sepiolite
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54—Particle size related information
    • C04B2235/5463—Particle size distributions
    • C04B2235/5472—Bimodal, multi-modal or multi-fraction

Definitions

  • the present invention relates to a process for producing a porous ceramic element for the diffusion of a liquid.
  • a watering device comprising a porous cone made of ceramic material connected to a tip made of polyvinyl chloride. This device is connected to a water reservoir, in particular a plastic bottle, then the cone is partially sunk into the ground to diffuse the water into the ground by gravity thanks to the porosity of the ceramic.
  • the porous cones must deliver a quantity of water adapted to the plant with which they are associated.
  • the porous cone models that fit on the same nozzle model, each model having a different theoretical water flow from the others, for example of the order of 7 cl per day, 20 cl per day , 30 cl per day.
  • Each cone is obtained from a slip cast in a mold under pressure. After demoulding, the raw cone is dried and then cooked. To modulate the porosity, the composition of the slip is adjusted.
  • each cone must be machined so that the outer bearing surface can be force fitted into an end piece.
  • This embodiment does not give full satisfaction because it does not make it possible to obtain a reliable throughput.
  • the present invention aims to overcome the drawbacks of the prior art by proposing a method for producing a porous ceramic element for the diffusion of a liquid making it possible to control the actual flow rate.
  • FIG. 1 there is shown a watering device for distributing water in a pot 10 filled with soil in which a plant 12 grows.
  • the invention is not limited to this application, the device being able to be implanted in any substrate in which one seeks to diffuse a liquid with a controlled rate.
  • the device comprises a porous ceramic element 14 partially sunk into the substrate secured to an end piece 16 to connect it to a removable reservoir 18 containing the liquid to be diffused into the substrate.
  • the liquid flows by gravity from the reservoir 18 towards the substrate thanks to the porosity of the element 14.
  • the porous element 14 comprises at its end a hollow conical portion 20 which is surmounted by a hollow substantially cylindrical portion 21, as illustrated in the picture 2 .
  • the porous element 14 has a substantially constant thickness.
  • longitudinal direction means the direction parallel to the axis of the conical portion 20 and to that of the cylindrical portion 21.
  • longitudinal plane means a plane containing the axis of the conical portion 20 and that of the cylindrical portion 21.
  • transverse plane is meant a plane perpendicular to the longitudinal direction.
  • the end piece 16 has a shape of revolution along the longitudinal axis and forms a conduit with, at a first end, means 22 for connecting with the porous ceramic element 14 and at the second end means for connecting 24 with the removable reservoir. 18.
  • the connecting means 24 must make it possible to quickly dissociate the removable tank 18.
  • the end piece 16 can comprise at the level of the second end a bore with a screw pitch making it possible to secure the tank 18 by screwing.
  • the connecting means 22 must limit the inadvertent separation of the end piece 16 and the porous element 14.
  • the end piece 16 may comprise at the first end a bore whose internal diameter is adapted to the external diameter of the porous element 14 in order to obtain a press fit of said porous element in the endpiece.
  • the tip is made at least at the first end of a material that is flexible enough to be able to compress slightly at the level of the connecting means 22.
  • This solution makes it possible to obtain a satisfactory fitting which tolerates a greater tolerance interval at the level the diameter of the seat of the fitted porous element.
  • the dimensional accuracy obtained at the end of the manufacturing process by pressure casting of a slip is satisfactory and does not require subsequent machining to reduce the tolerance interval.
  • the tip 16 can be made of SEBS (Styrene-Ethylene-Butylene-Styrene) with a Shore hardness of 90. This material is relatively elastic which makes it possible to compensate for the irregularities of the porous element 14 made of ceramic.
  • the relative flexibility of the tip material allows to force-fit the porous element 14 ensuring the seal.
  • the porous element 14 is obtained from a slip cast under pressure.
  • the element obtained at the end of the molding operation is then dried and then fired.
  • the porous element must have a suitable porosity to guarantee a given flow rate of liquid.
  • a first type of porous element has a flow rate of around 7 cl per day
  • a second type of porous element has a flow rate of around 20 cl per day
  • a third type of porous element has a flow rate of around 30 cl per day.
  • the porosity of the element 14 is determined according to the percentage of silicas and the particle size of the latter.
  • silica is used with a particle size distribution of the first type with about 30% fines with a diameter greater than 40 ⁇ m , and only 10% fines with a diameter greater than 75 ⁇ m .
  • the silica with the particle size distribution of the second type has a coarser particle size than the silica with the particle size distribution of the first type which makes it possible to increase the flow rate.
  • the percentage of silica with the particle size distribution of the first type, which is finer, is never zero and preferably greater than 10% to give the porous ceramic element 14 a suitable mechanical strength so as not to risk breaking it during mounting in the end piece 16.
  • the molding process under pressure as well as the firing of the porous elements 14 must not alter the value of the flow rate conferred by the percentage of at least two silicas with different particle sizes.
  • the molding of the porous element is carried out under pressure in a mold 26 illustrated in detail on the picture 3 .
  • This mold 26 comprises an upper part 28 providing a flat support surface 30 (parallel to a transverse plane) with for each porous element 14 a hollow shape 32 and a lower part 34 providing a flat support surface 36 (parallel to a transverse plane) with for each porous element 14 a projecting shape 38.
  • a space 40 is formed between the hollow shape 32 and the projecting shape 38 whose dimensions are adapted to obtain at the end of the process a porous element with the desired dimensions.
  • the lower part 34 comprises around the conical projecting shape 38 a channel 42 with a chamfer 43 to give the porous element a chamfer at the end of the cylindrical portion capable of being fitted into an end piece in order to facilitate this fitting.
  • the upper part 28 and the lower part 34 of the mold respectively comprise several recessed shapes 32 and several projecting shapes 38 which cooperate so as to obtain in a single molding operation several green porous elements.
  • At least the portion of the upper part 28 in which the recessed shapes are made is made of a porous resin.
  • the projecting shapes of the lower part 34 of the mold are made of a porous resin.
  • the recessed shapes of the upper part 28 and the projecting shapes of the lower part 34 are machined so as to guarantee good dimensional precision, the porous resin having a large shrinkage not making it possible to guarantee dimensional precision.
  • the mold comprises for each protruding shape 38 a slip supply 44 which opens at the top of the protruding shape 38.
  • the various power supplies 44 are connected to a central power supply 46 supplied by an injection pump 50 and controlled by a solenoid valve 52 for supplying slip.
  • the upper part 28 comprises air channels 54 which extend parallel to the longitudinal direction and open into a manifold 56 provided at the level of the face of the upper part opposite to the flat bearing surface 30.
  • the channels of air 54 are preferably blind and end near the flat bearing surface 30 or the surface forming the recessed shapes 32.
  • the air channels 54 preferably have a diameter of the order of 3 mm.
  • an air channel 54.1 is provided at the top of each hollow shape 32.
  • Air channels 54.2 are provided between two air channels 54.1 in a first direction and air channels 54.3 are provided between two 54.1 air channels in a direction perpendicular to the first.
  • Manifold 56 is connected to an exhaust solenoid valve 58 and an air supply solenoid valve 60.
  • the lower part 34 of the mold can comprise air channels opening into a manifold 62 connected to an exhaust solenoid valve 64 and to an air supply solenoid valve 66.
  • the manufacturing cycle for green porous elements is as follows.
  • the upper and lower parts are pressed against each other by exerting a clamping pressure.
  • the air collectors 56 and 62 are connected to the exhaust.
  • the solenoid valves 58 and 64 are in the on state and the solenoid valves 60 and 66 in the off state.
  • the slurry is then injected.
  • the porous resin of the mold allows the evacuation of water. After the spaces 40 have been filled at a given speed, the injection of the slip is stopped. After a given time, the solenoid valve 52 of the power supply is put in the off state. Next, exhaust solenoid valves 58 and 64 are turned off.
  • the upper part 28 of the mold is separated from the lower part 34 of the mold.
  • the air manifold 62 is connected to a supply of compressed air, the air supply solenoid valve 66 being in the on state.
  • the green porous elements are held in the upper part 28 of the mold.
  • a perforated plate is then placed under said upper part 28, then the air manifold of the upper part is connected to a compressed air supply in order to unmold the parts, the air supply solenoid valve 60 being in the state passing.
  • the perforated plate comprises a plurality of through holes with a diameter of between 1 and 4 mm.
  • This perforated plate must have an open rate of between 40 and 70% to ensure a good compromise between satisfactory evacuation of the water and not obtaining a mark on the raw porous elements.
  • the raw porous elements undergo a natural pre-drying by natural convection for example.
  • This cooking cycle is essential because it guarantees the homogeneous character of the porosity.
  • a passage oven is used.
  • the cooking cycle has a duration of the order of 90 min and comprises four phases, a first preheating phase at a temperature of the order of 900° C. for a duration of the order of 20 to 24 min, i.e. approximately 25% of the total duration, a second phase of temperature rise to a temperature of the order of 1160°C for a duration of the order of 10 to 12 min, i.e. approximately 12% of the total duration, a third phase corresponding to a plateau and maintenance at the temperature of the second phase for a period of 10 to 12 min, i.e.

Description

La présente invention se rapporte à un procédé de réalisation d'un élément poreux en céramique pour la diffusion d'un liquide.The present invention relates to a process for producing a porous ceramic element for the diffusion of a liquid.

On connait d'après le document WO-03/007697 un dispositif d'arrosage comprenant un cône poreux en matériau céramique relié à un embout en polychlorure de vinyle. Ce dispositif est relié à un réservoir d'eau, notamment une bouteille en plastique, puis le cône est partiellement enfoncé dans la terre pour diffuser par gravité l'eau dans la terre grâce à la porosité de la céramique.We know from the document WO-03/007697 a watering device comprising a porous cone made of ceramic material connected to a tip made of polyvinyl chloride. This device is connected to a water reservoir, in particular a plastic bottle, then the cone is partially sunk into the ground to diffuse the water into the ground by gravity thanks to the porosity of the ceramic.

Sur le plan fonctionnel, les cônes poreux doivent délivrer une quantité d'eau adaptée à la plante auxquels ils sont associés. Ainsi, il existe plusieurs modèles de cônes poreux qui s'adaptent sur le même modèle d'embout, chaque modèle ayant un débit d'eau théorique différent des autres, par exemple de l'ordre de 7 cl par jour, 20 cl par jour, 30 cl par jour.Functionally, the porous cones must deliver a quantity of water adapted to the plant with which they are associated. Thus, there are several porous cone models that fit on the same nozzle model, each model having a different theoretical water flow from the others, for example of the order of 7 cl per day, 20 cl per day , 30 cl per day.

Chaque cône est obtenu à partir d'une barbotine coulée dans un moule sous pression. Après démoulage, le cône cru est séché puis cuit. Pour moduler la porosité, on ajuste la composition de la barbotine.Each cone is obtained from a slip cast in a mold under pressure. After demoulding, the raw cone is dried and then cooked. To modulate the porosity, the composition of the slip is adjusted.

Compte tenu de la rigidité de l'embout et des précisions dimensionnelles obtenues à partir du procédé de moulage, chaque cône doit être usiné pour que la portée extérieure puisse être emboitée en force dans un embout.Given the rigidity of the end piece and the dimensional precision obtained from the molding process, each cone must be machined so that the outer bearing surface can be force fitted into an end piece.

Ce mode de réalisation ne donne pas pleinement satisfaction car il ne permet pas d'obtenir un débit fiable.This embodiment does not give full satisfaction because it does not make it possible to obtain a reliable throughput.

La présente invention vise à pallier aux inconvénients de l'art antérieur en proposant un procédé de réalisation d'un élément poreux en céramique pour la diffusion d'un liquide permettant de maîtriser le débit réel.The present invention aims to overcome the drawbacks of the prior art by proposing a method for producing a porous ceramic element for the diffusion of a liquid making it possible to control the actual flow rate.

A cet effet, l'invention est exposée dans le jeu de revendications joint.To this end, the invention is set out in the attached set of claims.

D'autres caractéristiques et avantages ressortiront de la description qui va suivre de l'invention, description donnée à titre d'exemple uniquement, en regard des dessins annexés sur lesquels :

  • la figure 1 est une vue en perspective d'un dispositif d'arrosage intégrant un élément poreux en céramique pour la diffusion d'un liquide implanté dans un pot de fleur,
  • la figure 2 est une section selon un plan longitudinal d'un élément poreux en céramique et d'un embout,
  • la figure 3 est une coupe illustrant deux parties d'un moule pour l'obtention d'un élément poreux en céramique,
  • la figure 4 est une représentation schématique d'une machine de coulage sous pression pour l'obtention d'éléments poreux en céramique,
  • la figure 5 est une vue de face de la partie supérieure du moule,
  • la figure 6 est une vue de face de la partie inférieure du moule,
  • la figure 7A est une vue de face illustrant une autre variante d'une partie supérieure d'un moule, et
  • la figure 7B est une coupe de la variante visible sur la figure 7A.
Other characteristics and advantages will emerge from the following description of the invention, description given by way of example only, with reference to the appended drawings in which:
  • the figure 1 is a perspective view of a watering device integrating a porous ceramic element for the diffusion of a liquid implanted in a flower pot,
  • the picture 2 is a section along a longitudinal plane of a porous ceramic element and a tip,
  • the picture 3 is a section illustrating two parts of a mold for obtaining a porous ceramic element,
  • the figure 4 is a schematic representation of a die-casting machine for obtaining porous ceramic elements,
  • the figure 5 is a front view of the upper part of the mould,
  • the figure 6 is a front view of the lower part of the mold,
  • the Figure 7A is a front view illustrating another variant of an upper part of a mould, and
  • the figure 7B is a cut of the variant visible on the Figure 7A .

Sur la figure 1, on a représenté un dispositif d'arrosage permettant de diffuser de l'eau dans un pot 10 rempli de terre dans lequel pousse une plante 12. Cependant, l'invention n'est pas limitée à cette application, le dispositif pouvant être implanté dans tout substrat dans lequel on cherche à diffuser un liquide avec un débit contrôlé.On the figure 1 , there is shown a watering device for distributing water in a pot 10 filled with soil in which a plant 12 grows. However, the invention is not limited to this application, the device being able to be implanted in any substrate in which one seeks to diffuse a liquid with a controlled rate.

De manière connue, le dispositif comprend un élément poreux en céramique 14 partiellement enfoncé dans le substrat solidaire d'un embout 16 pour le relier à un réservoir amovible 18 contenant le liquide à diffuser dans le substrat. Le liquide s'écoule par gravité du réservoir 18 vers le substrat grâce à la porosité de l'élément 14.In known manner, the device comprises a porous ceramic element 14 partially sunk into the substrate secured to an end piece 16 to connect it to a removable reservoir 18 containing the liquid to be diffused into the substrate. The liquid flows by gravity from the reservoir 18 towards the substrate thanks to the porosity of the element 14.

Pour permettre son enfoncement dans le substrat et garantir la diffusion du liquide, l'élément poreux 14 comprend au niveau de son extrémité une portion conique creuse 20 qui est surmontée d'une portion sensiblement cylindrique creuse 21, comme illustré sur la figure 2. De préférence, l'élément poreux 14 a une épaisseur sensiblement constante.To allow it to be driven into the substrate and guarantee the diffusion of the liquid, the porous element 14 comprises at its end a hollow conical portion 20 which is surmounted by a hollow substantially cylindrical portion 21, as illustrated in the picture 2 . Preferably, the porous element 14 has a substantially constant thickness.

Pour la suite de la description, on entend par direction longitudinale, la direction parallèle à l'axe de la portion conique 20 et à celui de la portion cylindrique 21. Par plan longitudinal, on entend un plan contenant l'axe de la portion conique 20 et celui de la portion cylindrique 21. Par plan transversal, on entend un plan perpendiculaire à la direction longitudinale.For the rest of the description, the term longitudinal direction means the direction parallel to the axis of the conical portion 20 and to that of the cylindrical portion 21. The term longitudinal plane means a plane containing the axis of the conical portion 20 and that of the cylindrical portion 21. By transverse plane is meant a plane perpendicular to the longitudinal direction.

L'embout 16 a une forme de révolution selon l'axe longitudinal et forme un conduit avec à une première extrémité des moyens de liaison 22 avec l'élément poreux 14 en céramique et à la seconde extrémité des moyens de liaison 24 avec le réservoir amovible 18.The end piece 16 has a shape of revolution along the longitudinal axis and forms a conduit with, at a first end, means 22 for connecting with the porous ceramic element 14 and at the second end means for connecting 24 with the removable reservoir. 18.

Les moyens de liaison 24 doivent permettre de dissocier rapidement le réservoir amovible 18. L'embout 16 peut comprendre au niveau de la seconde extrémité un alésage avec un pas de vis permettant de solidariser le réservoir 18 par vissage.The connecting means 24 must make it possible to quickly dissociate the removable tank 18. The end piece 16 can comprise at the level of the second end a bore with a screw pitch making it possible to secure the tank 18 by screwing.

Les moyens de liaison 22 doivent limiter la désolidarisation de manière intempestive de l'embout 16 et de l'élément poreux 14. L'embout 16 peut comprendre au niveau de la première extrémité un alésage dont le diamètre intérieur est adapté au diamètre extérieur de l'élément poreux 14 afin d'obtenir un emmanchement en force dudit élément poreux dans l'embout.The connecting means 22 must limit the inadvertent separation of the end piece 16 and the porous element 14. The end piece 16 may comprise at the first end a bore whose internal diameter is adapted to the external diameter of the porous element 14 in order to obtain a press fit of said porous element in the endpiece.

L'embout est réalisé au moins au niveau de la première extrémité en un matériau suffisamment souple pour pouvoir légèrement se comprimer au niveau des moyens de liaison 22. Cette solution permet d'obtenir un emmanchement satisfaisant qui tolère un intervalle de tolérance plus important au niveau du diamètre de la portée de l'élément poreux emmanché. La précision dimensionnelle obtenue à l'issue du procédé de fabrication par moulage sous pression d'une barbotine est satisfaisante et ne nécessite pas un usinage ultérieur pour réduire l'intervalle de tolérance.The tip is made at least at the first end of a material that is flexible enough to be able to compress slightly at the level of the connecting means 22. This solution makes it possible to obtain a satisfactory fitting which tolerates a greater tolerance interval at the level the diameter of the seat of the fitted porous element. The dimensional accuracy obtained at the end of the manufacturing process by pressure casting of a slip is satisfactory and does not require subsequent machining to reduce the tolerance interval.

L'embout 16 peut être réalisé en SEBS (Styrène-Ethylène-Butylène-Styrène) avec une dureté Shore de 90. Cette matière est relativement élastique ce qui permet de palier aux irrégularités de l'élément poreux 14 en céramique.The tip 16 can be made of SEBS (Styrene-Ethylene-Butylene-Styrene) with a Shore hardness of 90. This material is relatively elastic which makes it possible to compensate for the irregularities of the porous element 14 made of ceramic.

Cette solution permet de réduire fortement les coûts de fabrication en limitant les rebus au niveau de la fabrication des éléments poreux 14 en céramique qui ne sont plus usinés ultérieurement.This solution makes it possible to greatly reduce the manufacturing costs by limiting the scrap at the level of the manufacturing of the porous ceramic elements 14 which are no longer machined subsequently.

Selon un autre avantage, la relative souplesse du matériau de l'embout permet d'emmancher en force l'élément poreux 14 en assurant l'étanchéité.According to another advantage, the relative flexibility of the tip material allows to force-fit the porous element 14 ensuring the seal.

De manière connue, l'élément poreux 14 est obtenu à partir d'une barbotine coulée sous pression. L'élément obtenu à l'issue de l'opération de moulage est ensuite séché puis cuit.In a known manner, the porous element 14 is obtained from a slip cast under pressure. The element obtained at the end of the molding operation is then dried and then fired.

La composition de la barbotine est la suivante :

  • 20 à 35 % d'argile commercialisée sous la dénomination commerciale « Argile Stephan Schmidt 2100 »,
  • 10 à 40 % de silice,
  • 20 à 35 % de kaolin commercialisé sous la dénomination « Kaolin Soka 111 »,
  • 15 à 25 % de feldspath sodique,
  • de préférence, au moins un agent de défloculation,
  • de préférence, au moins un agent favorisant la prise et agglomérant les fines.
The composition of the slip is as follows:
  • 20 to 35% clay marketed under the trade name "Argile Stephan Schmidt 2100",
  • 10 to 40% silica,
  • 20 to 35% kaolin marketed under the name "Kaolin Soka 111",
  • 15 to 25% sodium feldspar,
  • preferably, at least one deflocculating agent,
  • preferably, at least one agent promoting the setting and agglomerating the fines.

Sur le plan pratique, l'élément poreux doit avoir une porosité adaptée pour garantir un débit de liquide donné.On a practical level, the porous element must have a suitable porosity to guarantee a given flow rate of liquid.

A titre d'exemple, on peut prévoir trois types d'éléments poreux avec des débits différents. Par exemple, un premier type d'éléments poreux a un débit de l'ordre de 7 cl par jour, un deuxième type d'éléments poreux a un débit de l'ordre de 20 cl par jour et un troisième type d'éléments poreux a un débit de l'ordre de 30 cl par jour.By way of example, three types of porous elements can be provided with different flow rates. For example, a first type of porous element has a flow rate of around 7 cl per day, a second type of porous element has a flow rate of around 20 cl per day and a third type of porous element has a flow rate of around 30 cl per day.

La porosité de l'élément 14 est déterminée en fonction du pourcentage de silices et de la granulométrie de ces dernières.The porosity of the element 14 is determined according to the percentage of silicas and the particle size of the latter.

Pour obtenir le débit intermédiaire, on utilise pour la silice de l'ordre de 40 % d'une silice avec une répartition granulométrique d'un premier type avec de l'ordre de 30% de fines avec un diamètre supérieur à 40 µm, et seulement 10% de fines avec un diamètre supérieur à 75 µm et 60 % d'une silice avec une répartition granulométrique d'un second type avec de l'ordre de 20% de fines avec un diamètre supérieur à 80 µm.To obtain the intermediate flow rate, use is made for the silica of the order of 40% of a silica with a particle size distribution of a first type with of the order of 30% of fines with a diameter greater than 40 μm , and only 10% of fines with a diameter greater than 75 µm and 60% of a silica with a particle size distribution of a second type with about 20% fines with a diameter greater than 80 µm .

Pour obtenir le débit le plus important, on utilise pour la silice de l'ordre de 30 % d'une silice avec une répartition granulométrique du premier type et 70 % d'une silice avec une répartition granulométrique du second type.To obtain the highest flow rate, use is made for the silica of the order of 30% of a silica with a particle size distribution of the first type and 70% of a silica with a particle size distribution of the second type.

Pour obtenir le débit le plus faible, on utilise uniquement la silice avec une répartition granulométrique du premier type avec de l'ordre de 30% de fines avec un diamètre supérieur à 40 µm, et seulement 10% de fines avec un diamètre supérieur à 75 µm.To obtain the lowest flow rate, only silica is used with a particle size distribution of the first type with about 30% fines with a diameter greater than 40 μm , and only 10% fines with a diameter greater than 75 µm .

La silice avec la répartition granulométrique du second type a une granulométrie plus grossière que la silice avec la répartition granulométrique du premier type ce qui permet d'augmenter le débit.The silica with the particle size distribution of the second type has a coarser particle size than the silica with the particle size distribution of the first type which makes it possible to increase the flow rate.

Ainsi, en ajustant le pourcentage d'au moins deux types de silices avec des granulométries différentes, il est possible d'ajuster le débit des éléments poreux 14.Thus, by adjusting the percentage of at least two types of silica with different grain sizes, it is possible to adjust the flow rate of the porous elements 14.

Le pourcentage de la silice avec la répartition granulométrique du premier type, plus fine, n'est jamais nul et de préférence supérieur à 10 % pour conférer à l'élément poreux 14 en céramique une résistance mécanique adaptée pour ne pas risquer de le casser lors du montage dans l'embout 16.The percentage of silica with the particle size distribution of the first type, which is finer, is never zero and preferably greater than 10% to give the porous ceramic element 14 a suitable mechanical strength so as not to risk breaking it during mounting in the end piece 16.

A titre d'exemple, pour le débit le plus faible, la barbotine a la composition suivante :

  • 30% (avec une précision de +/-5%) d'argile commercialisée sous la dénomination commerciale « Argile Stephan Schmidt 2100 »,
  • 33% (avec une précision de +/-5%) de kaolin commercialisé sous la dénomination « Kaolin Soka 111 »,
  • 15% (avec une précision de +/-5%) de silice du premier type,
  • 22% (avec une précision de +/-5%) de feldspath sodique, et
au moins un agent de défloculation et au moins un agent favorisant la prise et agglomérant les fines.By way of example, for the lowest flow rate, the slurry has the following composition:
  • 30% (with an accuracy of +/-5%) of clay marketed under the trade name "Argile Stephan Schmidt 2100",
  • 33% (with an accuracy of +/-5%) of kaolin marketed under the name "Kaolin Soka 111",
  • 15% (with an accuracy of +/-5%) of silica of the first type,
  • 22% (with an accuracy of +/-5%) sodium feldspar, and
at least one deflocculating agent and at least one agent promoting setting and agglomerating the fines.

Pour un débit intermédiaire, la barbotine a la composition suivante :

  • 25% (avec une précision de +/-5%) d'argile commercialisée sous la dénomination commerciale « Argile Stephan Schmidt 2100 »,
  • 27% (avec une précision de +/-5%) de kaolin commercialisé sous la dénomination « Kaolin Soka 111 »,
  • 12% (avec une précision de +/-5%) de silice du premier type,
  • 18% (avec une précision de +/-5%) de silice du second type,
  • 18% (avec une précision de +/-5%) de feldspath sodique, et
au moins un agent de défloculation et au moins un agent favorisant la prise et agglomérant les fines.For an intermediate flow, the slip has the following composition:
  • 25% (with an accuracy of +/-5%) of clay marketed under the trade name "Argile Stephan Schmidt 2100",
  • 27% (with an accuracy of +/-5%) of kaolin marketed under the name "Kaolin Soka 111",
  • 12% (with an accuracy of +/-5%) of silica of the first type,
  • 18% (with an accuracy of +/-5%) of silica of the second type,
  • 18% (with an accuracy of +/-5%) sodium feldspar, and
at least one deflocculating agent and at least one agent promoting setting and agglomerating the fines.

Pour le débit le plus important, la barbotine a la composition suivante :

  • 22% (avec une précision de +/-5%) d'argile commercialisée sous la dénomination commerciale « Argile Stephan Schmidt 2100 »,
  • 24% (avec une précision de +/-5%) de kaolin commercialisé sous la dénomination « Kaolin Soka 111 »,
  • 11% (avec une précision de +/-5%) de silice du premier type,
  • 27% (avec une précision de +/-5%) de silice du second type,
  • 16% (avec une précision de +/-5%) de feldspath sodique, et
au moins un agent de défloculation et au moins un agent favorisant la prise et agglomérant les fines.For the highest flow, the slurry has the following composition:
  • 22% (with an accuracy of +/-5%) of clay marketed under the trade name "Argile Stephan Schmidt 2100",
  • 24% (with an accuracy of +/-5%) of kaolin marketed under the name "Kaolin Soka 111",
  • 11% (with an accuracy of +/-5%) of silica of the first type,
  • 27% (with an accuracy of +/-5%) of silica of the second type,
  • 16% (with an accuracy of +/-5%) sodium feldspar, and
at least one deflocculating agent and at least one agent promoting setting and agglomerating the fines.

Le procédé de moulage sous pression ainsi que la cuisson des éléments poreux 14 ne doivent pas altérer la valeur du débit conféré par le pourcentage d'au moins deux silices avec des granulométries différentes.The molding process under pressure as well as the firing of the porous elements 14 must not alter the value of the flow rate conferred by the percentage of at least two silicas with different particle sizes.

Le moulage de l'élément poreux est réalisé sous pression dans un moule 26 illustré en détails sur la figure 3.The molding of the porous element is carried out under pressure in a mold 26 illustrated in detail on the picture 3 .

Ce moule 26 comprend une partie supérieure 28 offrant une surface plane d'appui 30 (parallèle à un plan transversal) avec pour chaque élément poreux 14 une forme en creux 32 et une partie inférieure 34 offrant une surface plane d'appui 36 (parallèle à un plan transversal) avec pour chaque élément poreux 14 une forme en saillie 38.This mold 26 comprises an upper part 28 providing a flat support surface 30 (parallel to a transverse plane) with for each porous element 14 a hollow shape 32 and a lower part 34 providing a flat support surface 36 (parallel to a transverse plane) with for each porous element 14 a projecting shape 38.

Lorsque les surfaces planes d'appui 30 et 36 sont en contact, un espace 40 est formé entre la forme en creux 32 et la forme en saillie 38 dont les dimensions sont adaptées pour obtenir en fin de procédé un élément poreux aux dimensions souhaitées.When the flat bearing surfaces 30 and 36 are in contact, a space 40 is formed between the hollow shape 32 and the projecting shape 38 whose dimensions are adapted to obtain at the end of the process a porous element with the desired dimensions.

Selon une variante améliorée illustrée sur la figure 2, pour chaque élément poreux 14, la partie inférieure 34 comprend autour de la forme en saillie conique 38 une rigole 42 avec un chanfrein 43 pour conférer à l'élément poreux un chanfrein au niveau de l'extrémité de la portion cylindrique susceptible d'être emmanchée dans un embout afin de favoriser cet emmanchement.According to an improved variant illustrated in the figure 2 , for each porous element 14, the lower part 34 comprises around the conical projecting shape 38 a channel 42 with a chamfer 43 to give the porous element a chamfer at the end of the cylindrical portion capable of being fitted into an end piece in order to facilitate this fitting.

La partie supérieure 28 et la partie inférieure 34 du moule comprennent respectivement plusieurs formes en creux 32 et plusieurs formes en saillie 38 qui coopèrent de manière à obtenir en une seule opération de moulage plusieurs éléments poreux crus.The upper part 28 and the lower part 34 of the mold respectively comprise several recessed shapes 32 and several projecting shapes 38 which cooperate so as to obtain in a single molding operation several green porous elements.

Au moins la portion de la partie supérieure 28 dans laquelle sont réalisées les formes en creux est réalisée en une résine poreuse. De préférence, les formes en saillie de la partie inférieure 34 du moule sont réalisées en une résine poreuse.At least the portion of the upper part 28 in which the recessed shapes are made is made of a porous resin. Preferably, the projecting shapes of the lower part 34 of the mold are made of a porous resin.

Les formes en creux de la partie supérieure 28 et les formes en saillie de la partie inférieure 34 sont usinées de manière à garantir une bonne précision dimensionnelle, la résine poreuse ayant un retrait important ne permettant pas de garantir la précision dimensionnelle.The recessed shapes of the upper part 28 and the projecting shapes of the lower part 34 are machined so as to guarantee good dimensional precision, the porous resin having a large shrinkage not making it possible to guarantee dimensional precision.

Le moule comprend pour chaque forme en saillie 38 une alimentation 44 en barbotine qui débouche au sommet de la forme en saillie 38.The mold comprises for each protruding shape 38 a slip supply 44 which opens at the top of the protruding shape 38.

De préférence, les différentes alimentations 44 sont reliées à une alimentation centrale 46 alimentée par une pompe d'injection 50 et commandée par une électrovanne 52 d'alimentation en barbotine.Preferably, the various power supplies 44 are connected to a central power supply 46 supplied by an injection pump 50 and controlled by a solenoid valve 52 for supplying slip.

Comme illustré sur la figure 5, la partie supérieure 28 comprend des canaux 54 d'air qui s'étendent parallèlement à la direction longitudinale et débouchent dans un collecteur 56 prévu au niveau de la face de la partie supérieure opposée à la surface plane d'appui 30. Les canaux d'air 54 sont de préférence borgnes et se terminent à proximité de la surface plane d'appui 30 ou de la surface formant les formes en creux 32.As illustrated on the figure 5 , the upper part 28 comprises air channels 54 which extend parallel to the longitudinal direction and open into a manifold 56 provided at the level of the face of the upper part opposite to the flat bearing surface 30. The channels of air 54 are preferably blind and end near the flat bearing surface 30 or the surface forming the recessed shapes 32.

Les canaux d'air 54 ont de préférence un diamètre de l'ordre de 3 mm.The air channels 54 preferably have a diameter of the order of 3 mm.

Selon un mode de réalisation, illustré sur la figure 5, un canal d'air 54.1 est prévu au niveau du sommet de chaque forme en creux 32. Des canaux d'air 54.2 sont prévus entre deux canaux d'air 54.1 selon une première direction et des canaux d'air 54.3 sont prévus entre deux canaux d'air 54.1 selon une direction perpendiculaire à la première.According to one embodiment, illustrated in the figure 5 , an air channel 54.1 is provided at the top of each hollow shape 32. Air channels 54.2 are provided between two air channels 54.1 in a first direction and air channels 54.3 are provided between two 54.1 air channels in a direction perpendicular to the first.

Selon une autre variante illustrée sur les figures 7A et 7B, il est possible de densifier les canaux d'air 54 prévus autour des formes en creux.According to another variant illustrated on the figures 7A and 7B , it is possible to densify the air channels 54 provided around the recessed shapes.

Le collecteur 56 est relié à une électrovanne d'échappement 58 et à une électrovanne d'alimentation en air 60.Manifold 56 is connected to an exhaust solenoid valve 58 and an air supply solenoid valve 60.

De la même manière, la partie inférieure 34 du moule peut comprendre des canaux d'air débouchant dans un collecteur 62 relié à une électrovanne d'échappement 64 et à une électrovanne d'alimentation en air 66.In the same way, the lower part 34 of the mold can comprise air channels opening into a manifold 62 connected to an exhaust solenoid valve 64 and to an air supply solenoid valve 66.

Le cycle de fabrication des éléments poreux crus est le suivant.The manufacturing cycle for green porous elements is as follows.

Dans un premier temps, les parties supérieure et inférieure sont plaquées l'une contre l'autre en exerçant une pression de serrage.Initially, the upper and lower parts are pressed against each other by exerting a clamping pressure.

Les collecteurs d'air 56 et 62 sont reliés à l'échappement. Ainsi, les électrovannes 58 et 64 sont à l'état passant et les électrovannes 60 et 66 à l'état non passant.The air collectors 56 and 62 are connected to the exhaust. Thus, the solenoid valves 58 and 64 are in the on state and the solenoid valves 60 and 66 in the off state.

On injecte alors la barbotine. La résine poreuse du moule permet l'évacuation de l'eau. Après le remplissage des espaces 40 à une vitesse donnée, l'injection de la barbotine est arrêtée. Après un temps donné, l'électrovanne 52 de l'alimentation est mise à l'état non passant. En suivant, les électrovannes d'échappement 58 et 64 sont mises à l'état non passant.The slurry is then injected. The porous resin of the mold allows the evacuation of water. After the spaces 40 have been filled at a given speed, the injection of the slip is stopped. After a given time, the solenoid valve 52 of the power supply is put in the off state. Next, exhaust solenoid valves 58 and 64 are turned off.

On arrête alors la pression hydraulique.The hydraulic pressure is then stopped.

Après une certaine durée, la partie supérieure 28 du moule est écartée de la partie inférieure 34 du moule. Pour faciliter le démoulage des pièces de la partie inférieure 34 du moule, on relie le collecteur d'air 62 à une alimentation en air comprimé, l'électrovanne d'alimentation en air 66 étant à l'état passant. En complément, on peut à l'aide d'une pompe à vide faire le vide dans le circuit de la partie supérieure du moule afin de faciliter le maintien des pièces dans cette partie du moule.After a period of time, the upper part 28 of the mold is separated from the lower part 34 of the mold. To facilitate the removal of the parts from the lower part 34 of the mould, the air manifold 62 is connected to a supply of compressed air, the air supply solenoid valve 66 being in the on state. In addition, it is possible, using a vacuum pump, to create a vacuum in the circuit of the upper part of the mold in order to facilitate the maintenance of the parts in this part of the mold.

Les éléments poreux crus sont maintenus dans la partie supérieure 28 du moule.The green porous elements are held in the upper part 28 of the mold.

On dispose alors sous ladite partie supérieure 28 une plaque ajourée, puis on relie le collecteur d'air de la partie supérieure à une alimentation en air comprimée afin de démouler les pièces, l'électrovanne d'alimentation en air 60 étant à l'état passant.A perforated plate is then placed under said upper part 28, then the air manifold of the upper part is connected to a compressed air supply in order to unmold the parts, the air supply solenoid valve 60 being in the state passing.

Pour ne pas marquer les pièces, la plaque ajourée comprend une pluralité de trous traversant d'un diamètre compris entre 1 et 4 mm. Cette plaque ajourée doit avoir un taux d'ouvert compris entre 40 et 70% pour assurer un bon compromis entre une évacuation satisfaisante de l'eau et ne pas obtenir de marque au niveau des éléments poreux crus.In order not to mark the parts, the perforated plate comprises a plurality of through holes with a diameter of between 1 and 4 mm. This perforated plate must have an open rate of between 40 and 70% to ensure a good compromise between satisfactory evacuation of the water and not obtaining a mark on the raw porous elements.

De préférence, les éléments poreux crus subissent un pré-séchage naturel par convection naturelle par exemple.Preferably, the raw porous elements undergo a natural pre-drying by natural convection for example.

En suivant, ils subissent un cycle de cuisson. Ce cycle de cuisson est primordial car il garantit le caractère homogène de la porosité.Next, they undergo a cooking cycle. This cooking cycle is essential because it guarantees the homogeneous character of the porosity.

Selon un mode de réalisation, on utilise un four à passage.According to one embodiment, a passage oven is used.

Le cycle de cuisson a une durée de l'ordre de 90 min et comprend quatre phases, une première phase de préchauffage à une température de l'ordre de 900°C pendant une durée de l'ordre de 20 à 24 min, soit environ 25% de la durée totale, une deuxième phase de montée en température jusqu'à une température de l'ordre de 1160°C pendant une durée de l'ordre de 10 à 12 min, soit environ 12% de la durée totale, une troisième phase correspondant à un pallier et un maintien à la température de la deuxième phase pendant une durée de 10 à 12 min, soit environ 12% de la durée totale, et une quatrième phase de refroidissement à une température de l'ordre de 740°C pendant une durée de 10 à 12 min, soit environ 12% de la durée totale, puis 30 à 36 min jusqu'à la sortie du four pour limiter les chocs thermiques.The cooking cycle has a duration of the order of 90 min and comprises four phases, a first preheating phase at a temperature of the order of 900° C. for a duration of the order of 20 to 24 min, i.e. approximately 25% of the total duration, a second phase of temperature rise to a temperature of the order of 1160°C for a duration of the order of 10 to 12 min, i.e. approximately 12% of the total duration, a third phase corresponding to a plateau and maintenance at the temperature of the second phase for a period of 10 to 12 min, i.e. approximately 12% of the total duration, and a fourth phase of cooling to a temperature of the order of 740° C for a period of 10 to 12 min, ie around 12% of the total duration, then 30 to 36 min until it comes out of the oven to limit thermal shocks.

Il est possible d'ajuster la porosité en faisant varier la température des deuxième et troisième phases et la durée desdites phases. Ainsi, il est possible d'augmenter la porosité des éléments poreux en réduisant la durée d'au moins une des phases 2 et 3 et/ou en réduisant la température des phases 2 et 3.It is possible to adjust the porosity by varying the temperature of the second and third phases and the duration of said phases. Thus, it is possible to increase the porosity of the porous elements by reducing the duration of at least one of phases 2 and 3 and/or by reducing the temperature of phases 2 and 3.

Claims (2)

  1. A method for making a porous ceramic element for water diffusion for spraying, said method comprising a step of die casting a slurry and then a firing step, characterised in that the slurry comprises from 10 to 40% of silicas of which 30 to 100% of a silica with a particle size distribution of a first type and 0 to 70% of a silica with a particle size distribution of a second type with a percentage of fines of large diameter greater than the particle size distribution of the first type, the silica with a particle size distribution of the first type comprising 30% of fines with a diameter greater than 40 µm, and only 10% of fines with a diameter greater than 75 µm, the silica with a particle size distribution of the second type comprising 20% of fines with a diameter greater than 80 µm, and in that the slurry further comprises 20 to 35% of clay, 20 to 35% of kaolin and 15 to 25% of sodium feldspar.
  2. The method for making a porous ceramic element according to the preceding claim, characterised in that the firing step comprises four phases, a first preheating phase at a temperature of 900°C, a second temperature rise phase up to a temperature of 1160°C, a third phase corresponding to a plateau and maintaining the temperature of the second phase and a fourth cooling phase at a temperature of 740°C to limit heat shocks.
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